HRID1076893

反应详情

EQUATION

反应方程式

HRID 1076893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 13.0 g (0.034 mole) of 2,7-bis(3-chloropropionyl)thioxanthene, 1 g of potassium iodide, 75 ml of diethylamine and 75 ml of tetrahydrofuran was allowed to stand for 72 hours and filtered. The residue was washed with tetrahydrofuran, evaporated to dryness then dissolved in ethanol. The solution was treated with ethanolic HCl, diluted with diethyl ether and the resulting solid was filtered off, recrystallized from methanol and diethyl ether and hydrated in a constant humidity chamber to give the desired product. M.P. 137°-140°C.

WORKUP

后处理

  1. filtrationfiltered
  2. washThe residue was washed with tetrahydrofuran
  3. customevaporated to dryness
  4. dissolutionthen dissolved in ethanol
  5. additionThe solution was treated with ethanolic HCl
  6. additiondiluted with diethyl ether
  7. filtrationthe resulting solid was filtered off
  8. customrecrystallized from methanol and diethyl ether and hydrated in a constant humidity chamber